반응 #80668

ord-cb646b4ed9e74716b41f57c77ae11bab

용매

반응 조건

온도
30°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타fitted with mechanical stirrer
  2. 2
    기타The organic phase is separated off
  3. 3
    추출The water phase is extracted with ethyl acetate
  4. 4
    세척The two organic phases are washed with sodium chloride-saturated water
  5. 5
    건조dried over sodium sulfate
  6. 6
    기타evaporated on a Rotavap

실험 절차

100 g (2.5 mol) of sodium hydroxide are dissolved in 100 ml of water in a 750 ml sulfonation flask fitted with mechanical stirrer, thermometer, dropping funnel and condenser. 71.9 g (0.25 mol) of 1-octyloxy-2,2,6,6-tetramethyl-4-hydroxypiperidine and 16.1 g (0.05 mol) of tetrabutylammonium bromide are added at 20° C. The mixture is warmed to 30° C. with vigorous stirring. A solution of 277.5 g (3 mol) of epichlorohydrin and 71.9 g (0.25 mol) of 1-octyloxy-2,2,6,6-tetramethyl-4-hydroxypiperidine is then added dropwise at 35° C. over the course of 75 minutes. The reaction solution is stirred at room temperature for 16 hours and poured onto 1 kg of ice and 100 g of sodium bicarbonate. The organic phase is separated off. The water phase is extracted with ethyl acetate. The two organic phases are washed with sodium chloride-saturated water, dried over sodium sulfate and evaporated on a Rotavap.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05616637uspto-grants-1997_04